CN106379948B - Method for preparing nano cobalt manganese oxyhydroxide - Google Patents
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- GYVYCYGQNBTVDM-UHFFFAOYSA-N O(O)O.[Mn].[Co] Chemical compound O(O)O.[Mn].[Co] GYVYCYGQNBTVDM-UHFFFAOYSA-N 0.000 title claims abstract description 33
- 238000000034 method Methods 0.000 title claims abstract description 27
- 239000011259 mixed solution Substances 0.000 claims abstract description 23
- 238000006243 chemical reaction Methods 0.000 claims abstract description 15
- 230000001590 oxidative effect Effects 0.000 claims abstract description 14
- 229940011182 cobalt acetate Drugs 0.000 claims abstract description 13
- QAHREYKOYSIQPH-UHFFFAOYSA-L cobalt(II) acetate Chemical compound [Co+2].CC([O-])=O.CC([O-])=O QAHREYKOYSIQPH-UHFFFAOYSA-L 0.000 claims abstract description 13
- 229940071125 manganese acetate Drugs 0.000 claims abstract description 13
- UOGMEBQRZBEZQT-UHFFFAOYSA-L manganese(2+);diacetate Chemical compound [Mn+2].CC([O-])=O.CC([O-])=O UOGMEBQRZBEZQT-UHFFFAOYSA-L 0.000 claims abstract description 13
- 238000001035 drying Methods 0.000 claims abstract description 6
- 238000007254 oxidation reaction Methods 0.000 claims abstract description 6
- 238000005406 washing Methods 0.000 claims abstract description 6
- 239000007789 gas Substances 0.000 claims description 13
- 239000011572 manganese Substances 0.000 claims description 10
- QAOWNCQODCNURD-UHFFFAOYSA-N Sulfuric acid Chemical compound OS(O)(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-N 0.000 claims description 8
- 239000002245 particle Substances 0.000 claims description 7
- 239000000126 substance Substances 0.000 claims description 6
- CBENFWSGALASAD-UHFFFAOYSA-N Ozone Chemical compound [O-][O+]=O CBENFWSGALASAD-UHFFFAOYSA-N 0.000 claims description 5
- 238000005273 aeration Methods 0.000 claims description 3
- KZBUYRJDOAKODT-UHFFFAOYSA-N Chlorine Chemical compound ClCl KZBUYRJDOAKODT-UHFFFAOYSA-N 0.000 claims description 2
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 claims 1
- 239000001301 oxygen Substances 0.000 claims 1
- 229910052760 oxygen Inorganic materials 0.000 claims 1
- 238000002360 preparation method Methods 0.000 abstract description 5
- 230000015572 biosynthetic process Effects 0.000 abstract description 4
- 238000003786 synthesis reaction Methods 0.000 abstract description 4
- 239000002994 raw material Substances 0.000 abstract description 3
- HBBGRARXTFLTSG-UHFFFAOYSA-N Lithium ion Chemical compound [Li+] HBBGRARXTFLTSG-UHFFFAOYSA-N 0.000 abstract description 2
- 239000003990 capacitor Substances 0.000 abstract description 2
- 229910001416 lithium ion Inorganic materials 0.000 abstract description 2
- 239000000047 product Substances 0.000 description 15
- 239000010941 cobalt Substances 0.000 description 7
- 229910017052 cobalt Inorganic materials 0.000 description 7
- GUTLYIVDDKVIGB-UHFFFAOYSA-N cobalt atom Chemical compound [Co] GUTLYIVDDKVIGB-UHFFFAOYSA-N 0.000 description 7
- PWHULOQIROXLJO-UHFFFAOYSA-N Manganese Chemical compound [Mn] PWHULOQIROXLJO-UHFFFAOYSA-N 0.000 description 4
- 238000001514 detection method Methods 0.000 description 4
- 229910052748 manganese Inorganic materials 0.000 description 4
- -1 manganese oxide compound Chemical class 0.000 description 4
- 239000002244 precipitate Substances 0.000 description 4
- 239000000243 solution Substances 0.000 description 4
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 4
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 description 3
- ZBYYWKJVSFHYJL-UHFFFAOYSA-L cobalt(2+);diacetate;tetrahydrate Chemical compound O.O.O.O.[Co+2].CC([O-])=O.CC([O-])=O ZBYYWKJVSFHYJL-UHFFFAOYSA-L 0.000 description 3
- 239000008367 deionised water Substances 0.000 description 3
- 229910021641 deionized water Inorganic materials 0.000 description 3
- 229940082328 manganese acetate tetrahydrate Drugs 0.000 description 3
- CESXSDZNZGSWSP-UHFFFAOYSA-L manganese(2+);diacetate;tetrahydrate Chemical compound O.O.O.O.[Mn+2].CC([O-])=O.CC([O-])=O CESXSDZNZGSWSP-UHFFFAOYSA-L 0.000 description 3
- 238000002441 X-ray diffraction Methods 0.000 description 2
- 229910001429 cobalt ion Inorganic materials 0.000 description 2
- XLJKHNWPARRRJB-UHFFFAOYSA-N cobalt(2+) Chemical compound [Co+2] XLJKHNWPARRRJB-UHFFFAOYSA-N 0.000 description 2
- AMWRITDGCCNYAT-UHFFFAOYSA-L manganese oxide Inorganic materials [Mn].O[Mn]=O.O[Mn]=O AMWRITDGCCNYAT-UHFFFAOYSA-L 0.000 description 2
- 238000004519 manufacturing process Methods 0.000 description 2
- 239000007800 oxidant agent Substances 0.000 description 2
- 238000001556 precipitation Methods 0.000 description 2
- MYMOFIZGZYHOMD-UHFFFAOYSA-N Dioxygen Chemical compound O=O MYMOFIZGZYHOMD-UHFFFAOYSA-N 0.000 description 1
- 229910008090 Li-Mn-O Inorganic materials 0.000 description 1
- 229910006369 Li—Mn—O Inorganic materials 0.000 description 1
- RHBREZMHGBURNU-UHFFFAOYSA-M O[Mn]O[Co] Chemical compound O[Mn]O[Co] RHBREZMHGBURNU-UHFFFAOYSA-M 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 239000003153 chemical reaction reagent Substances 0.000 description 1
- 150000001868 cobalt Chemical class 0.000 description 1
- 150000001875 compounds Chemical class 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 229910001882 dioxygen Inorganic materials 0.000 description 1
- 230000005518 electrochemistry Effects 0.000 description 1
- 238000000349 field-emission scanning electron micrograph Methods 0.000 description 1
- 238000000445 field-emission scanning electron microscopy Methods 0.000 description 1
- 150000004679 hydroxides Chemical class 0.000 description 1
- 239000007788 liquid Substances 0.000 description 1
- 229910001437 manganese ion Inorganic materials 0.000 description 1
- 239000002086 nanomaterial Substances 0.000 description 1
- 239000002105 nanoparticle Substances 0.000 description 1
- 230000006911 nucleation Effects 0.000 description 1
- 238000010899 nucleation Methods 0.000 description 1
- 230000003647 oxidation Effects 0.000 description 1
- 239000002243 precursor Substances 0.000 description 1
- 150000003839 salts Chemical class 0.000 description 1
- 229910052596 spinel Inorganic materials 0.000 description 1
- 239000011029 spinel Substances 0.000 description 1
- 238000012795 verification Methods 0.000 description 1
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01G—COMPOUNDS CONTAINING METALS NOT COVERED BY SUBCLASSES C01D OR C01F
- C01G51/00—Compounds of cobalt
-
- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01G—CAPACITORS; CAPACITORS, RECTIFIERS, DETECTORS, SWITCHING DEVICES, LIGHT-SENSITIVE OR TEMPERATURE-SENSITIVE DEVICES OF THE ELECTROLYTIC TYPE
- H01G11/00—Hybrid capacitors, i.e. capacitors having different positive and negative electrodes; Electric double-layer [EDL] capacitors; Processes for the manufacture thereof or of parts thereof
- H01G11/22—Electrodes
- H01G11/30—Electrodes characterised by their material
- H01G11/46—Metal oxides
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- H01—ELECTRIC ELEMENTS
- H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
- H01M10/00—Secondary cells; Manufacture thereof
- H01M10/05—Accumulators with non-aqueous electrolyte
- H01M10/052—Li-accumulators
- H01M10/0525—Rocking-chair batteries, i.e. batteries with lithium insertion or intercalation in both electrodes; Lithium-ion batteries
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
- H01M4/00—Electrodes
- H01M4/02—Electrodes composed of, or comprising, active material
- H01M4/36—Selection of substances as active materials, active masses, active liquids
- H01M4/48—Selection of substances as active materials, active masses, active liquids of inorganic oxides or hydroxides
- H01M4/52—Selection of substances as active materials, active masses, active liquids of inorganic oxides or hydroxides of nickel, cobalt or iron
- H01M4/523—Selection of substances as active materials, active masses, active liquids of inorganic oxides or hydroxides of nickel, cobalt or iron for non-aqueous cells
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Abstract
The invention discloses a method for preparing nanometer cobalt manganese oxyhydroxide, which comprises the following steps: (1) adjusting the pH value of the mixed solution of manganese acetate and cobalt acetate to 2.5-6; (2) and (2) introducing oxidizing gas into the mixed solution obtained in the step (1) to perform oxidation reaction, and centrifuging, washing and drying after reaction to obtain the nano cobalt manganese oxyhydroxide. The preparation method can be used for obtaining the nano cobalt manganese oxyhydroxide by one-step processing, and the nano cobalt manganese oxyhydroxide can be applied to related fields such as super capacitors, lithium ion batteries and the like. The preparation method has the advantages of cheap and easily-obtained raw materials, low cost, simple and easily-realized synthesis process, stable product quality, good process repeatability, reaction completion in a short time and high efficiency.
Description
Technical Field
The invention belongs to the field of nano materials, and particularly relates to a method for preparing nano cobalt manganese oxyhydroxide.
Background
The hydroxide compounds of manganese and cobalt have very important application in the fields of electrochemistry, batteries, electrochromism and the like. The hydroxyl manganese cobalt oxide can also be used as a precursor of a Li-Mn-O spinel structure and a manganese oxide compound with cobalt, and the manganese oxide compound with cobalt has very excellent performance in the aspects of secondary batteries and supercapacitors, and has been widely concerned by the scientific and industrial fields. Chinese patent application 201210578760.1 discloses a method for preparing trace manganese-doped cobalt oxyhydroxide, which comprises adding precipitant (KOH, NaOH, etc.) and oxidant (compressed air) into cobalt salt and M salt to synthesize trace manganese-containing cobalt oxyhydroxide, wherein the addition of precipitant and oxidant in the synthesis process can cause non-uniformity of reaction, resulting in poor product stability, requiring a long period of time for reaction, and having low efficiency, which is not suitable for mass production. Therefore, it is necessary to research a preparation method of manganese cobalt oxyhydroxide with simple and easily realized synthesis process, stable product quality and good process repeatability.
Disclosure of Invention
The technical problem to be solved by the invention is to overcome the defects and shortcomings mentioned in the background technology and provide a method for preparing nano cobalt manganese oxyhydroxide.
In order to solve the technical problems, the technical scheme provided by the invention is as follows:
a method for preparing nanometer cobalt manganese oxyhydroxide comprises the following steps:
(1) adjusting the pH value of the mixed solution of manganese acetate and cobalt acetate to 2.5-6;
(2) and (2) introducing oxidizing gas into the mixed solution obtained in the step (1) to perform oxidation reaction, and centrifuging, washing and drying after reaction to obtain the nano cobalt manganese oxyhydroxide.
Through repeated research and experimental verification, the applicant finds that when the pH value of the mixed solution is lower than 2.5, cobalt ions are difficult to oxidize and precipitate, only a small amount of cobalt precipitates in a short time, and the reaction efficiency is too low; when the pH value is higher than 6, the reaction rate is too fast, and the particle size of the product is difficult to control; it was also found that Co is present at the same pH2+Higher oxidation potential and precipitation than Mn2+The two precipitates are different in the same time, so that the atomic ratio of cobalt and manganese in the product can be adjusted by adjusting the pH value, and the content of doped cobalt can be changed.
In the above method, preferably, the chemical formula of the nano cobalt manganese oxyhydroxide is (Co)xMn1-x) OOH, wherein x is more than 0 and less than 1; the nano cobalt manganese oxyhydroxide is spherical, and the average particle size is 180 nm-200 nm.
In the method, preferably, the concentration of manganese acetate and cobalt acetate in the mixed solution of manganese acetate and cobalt acetate is 0.01 mol/L-0.02 mol/L.
In the above method, the oxidizing gas is preferably chlorine gas or a mixed gas of ozone and oxygen gas.
In the above method, the time of the oxidation reaction in the step (2) is preferably 45 to 75 min.
Preferably, in the step (2), oxidizing gas is introduced into the mixed solution at 25-70 ℃, the reaction temperature is controlled at 25-70 ℃, the nucleation and growth rates of manganese and cobalt can be changed, the particle size of the product is adjusted, and the precipitation rate is adjusted, so that the product is nanoparticles; the temperature in the reaction process is lower than 25 ℃, the reaction becomes slower, and the production efficiency is low; the reaction temperature is higher than 70 ℃, the reaction is rapid, and the water in the solution is seriously volatilized, which is not beneficial to the control of the grain size and the stability of the system.
In the above method, preferably, in the step (2), the oxidizing gas is introduced into the mixed solution through an aeration head. The oxidizing gas can form dispersed small bubbles in the solution through the aeration head, the oxidizing gas is uniformly dispersed in the liquid, and then the oxidizing gas reacts with manganese ions and cobalt ions in the solution to generate precipitates, so that the reaction is more sufficient.
Compared with the prior art, the invention has the advantages that:
(1) the preparation method can be used for obtaining the nano cobalt manganese oxyhydroxide by one-step processing, and the nano cobalt manganese oxyhydroxide can be applied to related fields such as super capacitors, lithium ion batteries and the like.
(2) The preparation method has the advantages of cheap and easily-obtained raw materials, low cost, simple and easily-realized synthesis process, stable product quality, good process repeatability, reaction completion in a short time and high efficiency.
Drawings
Fig. 1 is an XRD pattern of nano cobalt manganese oxyhydroxide prepared in example 1 of the present invention.
FIG. 2 is an FESEM image of nano cobalt manganese oxyhydroxide prepared in example 2 of the invention.
Detailed Description
In order to facilitate an understanding of the invention, the invention will be described more fully and in detail below with reference to the accompanying drawings and preferred embodiments, but the scope of the invention is not limited to the specific embodiments below.
Unless otherwise defined, all terms of art used hereinafter have the same meaning as commonly understood by one of ordinary skill in the art. The terminology used herein is for the purpose of describing particular embodiments only and is not intended to limit the scope of the present invention.
Unless otherwise specifically stated, various raw materials, reagents, instruments, equipment and the like used in the present invention are commercially available or can be prepared by existing methods.
Example 1:
the invention relates to a method for preparing nanometer cobalt manganese oxyhydroxide, which comprises the following steps:
(1) dissolving manganese acetate tetrahydrate and cobalt acetate tetrahydrate in 200mL of deionized water to prepare a mixed solution of manganese acetate and cobalt acetate, wherein the concentrations of the manganese acetate and the cobalt acetate are both 0.0125 mol/L;
(2) adjusting the pH value of the mixed solution to 2.5 by using dilute sulfuric acid;
(3) and (3) introducing ozone into the mixed solution treated in the step (2) at 35 ℃, reacting for 1h, centrifuging, washing, and finally drying at 80 ℃ to obtain a nano cobalt manganese oxyhydroxide product.
The XRD pattern of the nano-cobalt manganese oxyhydroxide product prepared in this example is shown in FIG. 1, which shows that the product is cobalt manganese oxyhydroxide with a chemical formula of (Co)a,Mn1-a) OOH, the number of the standard card is JCPDS 42-1316; the nano cobalt manganese oxyhydroxide prepared by the embodiment is spherical, and the particle size is about 181 nm; XPS detection further shows that the chemical formula of the compound is (Co)0.15Mn0.85)OOH。
The nano cobalt manganese oxyhydroxide prepared in the embodiment is prepared into an electrode slice, and constant-current charge-discharge detection is carried out in 6mol/L KOH solution, and the measured specific capacity is 707F/g.
Example 2:
the invention relates to a method for preparing nanometer cobalt manganese oxyhydroxide, which comprises the following steps:
(1) dissolving manganese acetate tetrahydrate and cobalt acetate tetrahydrate in 200mL of deionized water to prepare a mixed solution of manganese acetate and cobalt acetate, wherein the concentrations of the manganese acetate and the cobalt acetate are both 0.0125 mol/L;
(2) adjusting the pH value of the mixed solution to 3.5 by using dilute sulfuric acid;
(3) and (3) introducing ozone into the mixed solution treated in the step (2) at 35 ℃, reacting for 45min, centrifuging, washing, and finally drying at 80 ℃ to obtain a nano cobalt manganese oxyhydroxide product.
The FESEM of the nano-cobalt manganese oxyhydroxide product prepared in this example is shown in fig. 2, which shows that the nano-cobalt manganese oxyhydroxide prepared in this example is spherical and has a particle size of about 200 nm; the chemical formula of the nano cobalt manganese oxyhydroxide product of the embodiment is shown as (Co) through XRD and XPS detection0.27Mn0.73)OOH。
Example 3:
the invention relates to a method for preparing nanometer cobalt manganese oxyhydroxide, which comprises the following steps:
(1) dissolving manganese acetate tetrahydrate and cobalt acetate tetrahydrate in 200mL of deionized water to obtain a mixed solution of manganese acetate and cobalt acetate (the concentration of manganese acetate in the mixed solution is 0.0125mol/L, and the concentration of cobalt acetate is 0.025 mol/L);
(2) adjusting the pH value of the mixed solution to 2.5 by using dilute sulfuric acid;
(3) and (3) introducing ozone into the mixed solution treated in the step (2) at 70 ℃, reacting for 1h, centrifuging, washing, and finally drying at 80 ℃ to obtain a nano cobalt manganese oxyhydroxide product. The nano cobalt manganese oxyhydroxide prepared by the embodiment is spherical, and the particle size is about 123 nm; the chemical formula of the nano cobalt manganese oxyhydroxide product of the embodiment is shown as (Co) through XRD and XPS detection0.48Mn0.52)OOH。
Claims (4)
1. The method for preparing the nano cobalt manganese oxyhydroxide is characterized by comprising the following steps of:
(1) adjusting the pH value of the mixed solution of manganese acetate and cobalt acetate to 2.5-6 by using dilute sulfuric acid;
(2) introducing oxidizing gas into the mixed solution obtained in the step (1) to perform oxidation reaction, and centrifuging, washing and drying after reaction to obtain the nano cobalt manganese oxyhydroxide;
the chemical formula of the nano cobalt manganese oxyhydroxide is (Co)xMn1-x) OOH, wherein x is more than 0 and less than 1; the nano cobalt manganese oxyhydroxide is spherical, and the average particle size is 180 nm-200 nm;
in the mixed solution of the manganese acetate and the cobalt acetate, the concentrations of the manganese acetate and the cobalt acetate are both 0.01 mol/L-0.02 mol/L; the time of the oxidation reaction is 45 min-75 min.
2. The method of claim 1, wherein the oxidizing gas is chlorine gas or a mixed gas of ozone and oxygen.
3. The method according to any one of claims 1 to 2, wherein in the step (2), an oxidizing gas is introduced into the mixed solution at a temperature of 25 ℃ to 70 ℃.
4. The method according to any one of claims 1 to 2, wherein in the step (2), the oxidizing gas is introduced into the mixed solution through an aeration head.
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| CN101127398A (en) * | 2007-06-28 | 2008-02-20 | 河南师范大学 | A ball hydroxide oxidated Ni-Co-Mn and its making method |
| CN100577576C (en) * | 2007-04-20 | 2010-01-06 | 南京大学 | Simple method for ozone oxidation preparation of alpha-FeOOH, beta-MnO2 and Co3O4 nano material |
| CN103904323A (en) * | 2012-12-28 | 2014-07-02 | 北京当升材料科技股份有限公司 | Preparation method for spherical cobalt oxyhydroxide |
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|---|---|---|---|---|
| CN100577576C (en) * | 2007-04-20 | 2010-01-06 | 南京大学 | Simple method for ozone oxidation preparation of alpha-FeOOH, beta-MnO2 and Co3O4 nano material |
| CN101127398A (en) * | 2007-06-28 | 2008-02-20 | 河南师范大学 | A ball hydroxide oxidated Ni-Co-Mn and its making method |
| CN103904323A (en) * | 2012-12-28 | 2014-07-02 | 北京当升材料科技股份有限公司 | Preparation method for spherical cobalt oxyhydroxide |
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| 含钴溶液臭氧氧化沉淀及其在冶金中的应用研究;辛云涛;《中国优秀硕士学位论文全文数据库 工程科技Ⅰ辑》;20150315;56-58页 * |
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